CN102312294A - Additive used for monocrystalline silicon wafer alkaline flocking and application method thereof - Google Patents
Additive used for monocrystalline silicon wafer alkaline flocking and application method thereof Download PDFInfo
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- CN102312294A CN102312294A CN201110264998A CN201110264998A CN102312294A CN 102312294 A CN102312294 A CN 102312294A CN 201110264998 A CN201110264998 A CN 201110264998A CN 201110264998 A CN201110264998 A CN 201110264998A CN 102312294 A CN102312294 A CN 102312294A
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- wool
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Abstract
The invention relates to an additive used for monocrystalline silicon wafer alkaline flocking and an application method thereof, belonging to the technical field of solar batteries. The additive is prepared by the following components: ethanolamine, polyphosphate, sodium dodecylbenzene sulfonate, sodium hydroxide and water. A flocking agent is prepared through the following steps: (1) dissolving sodium hydroxide in deionized water so as to obtain alkaline flocking liquid; (2) adding the additive motioned above into the alkaline flocking liquid to obtain the flocking agent. During flocking, monocrystalline silicon wafers used for solar batteries are immersed in the flocking agent with temperature controlled to be 75 to 85 DEG C and flocking time controlled to be 15 to 18 minutes. The additive used for monocrystalline silicon wafer alkaline flocking in the invention enables flocking reaction time to be shortened and productivity to be enhanced; prepared texture surface pyramids have a uniform size and low reflectivity; the additive is applicable to solar battery silicon wafer alkaline flocking of different specifications and meets the purpose of industrial production.
Description
Technical field
The present invention relates to a kind of additive and method of use thereof that is used for the making herbs into wool of monocrystalline silicon piece alkali, belong to the manufacture of solar cells technical field.
Background technology
In the preparation technology of mono-crystalline silicon solar, often utilize alkaline solution different to each crystal face erosion rate, form the matte of similar " pyramid " shape at silicon chip surface.
The matte growing principle: at high temperature, following chemical reaction takes place in silicon and alkali:
Si+2OH
-+H
2O?=?SiO
3 2- +2H
2
For crystalline silicon, because the atomic density of each crystal face is different, the velocity contrast of reacting with alkali is very big, just our (110) face (111) of saying usually thus the corrosion of face forms the matte of similar " pyramid " shape on the surface.Effectively suede structure can effectively strengthen the absorption of silicon chip to the incident sunshine, improves photogenerated current density, thereby improves Solar cell performance and efficient.The making herbs into wool effect is mainly reflected in pyramid size and uniformity coefficient, and the pyramid size that general technology is produced is between 5-10 μ m, and the pyramid size is inhomogeneous, and has the space between the adjacent pyramid.
At present; Producing Woolen-making liquid commonly used in the industry is sodium hydroxide, water glass, Virahol, deionized water composition; The effect of this Woolen-making liquid is undesirable, and in silicon chip making herbs into wool production process, solution can lose efficacy; Thereby cause the production technique fluctuation, failure reasons is continuous consumption and the Na of NaOH in the reaction process
2SiO
3Continuous generation, cause reactant-OH concentration to reduce, and silicon chip surface can't with the enough exposure rates of its acquisition; And owing to be reflected at about high temperature 80 degree and carry out, vigorous reaction often takes place produce great amount of bubbles, need constantly to replenish the raindrop seal that Virahol reduces silicon chip surface, and the gained matte is unsatisfactory.Traditional technology generally is through adding the carrying out that water glass and IPA (Virahol) come inhibited reaction; The control speed of reaction, the matte pyramid structure that generates like this is inhomogeneous, and making herbs into wool stability is bad; Often can see finger-marks or hickie etc., more difficult controls reaction speed.
Summary of the invention
For addressing the above problem, the present invention provides a kind of pyramid size that can make to be controlled between 1 ~ 3 μ m, does not have the additive and the method for use thereof that are used for the making herbs into wool of monocrystalline silicon piece alkali in space between the even and adjacent pyramid of pyramid size.
For realizing above-mentioned purpose, the technical scheme that the present invention adopted is:
A kind of additive that is used for the making herbs into wool of monocrystalline silicon piece alkali, formulated by following component: thanomin (2-monoethanolamine), poly-phosphate, X 2073, sodium hydroxide, water.
As the further setting of such scheme, the mol ratio between said thanomin, poly-phosphate, X 2073, sodium hydroxide, the water is 12 ~ 25:5 ~ 15:1 ~ 10:1 ~ 5:20 ~ 100.
Mol ratio between said thanomin, poly-phosphate, X 2073, sodium hydroxide, the water is 15 ~ 20:8 ~ 12:3 ~ 8:1 ~ 3:80 ~ 100.
Said water is deionized water.
Said poly-phosphate can be any one in Rapisol (Potassium tripolyphosphate), sodium polyphosphate (tripoly phosphate sodium STPP, sodium tetrapolyphosphate), the ammonium polyphosphate (n=10 ~ 20, water-soluble).
A kind of Wool-making agent that is used for the making herbs into wool of monocrystalline silicon piece alkali, formulated by following steps:
⑴ be dissolved in sodium hydroxide in the deionized water, obtains alkaline Woolen-making liquid, and wherein sodium hydroxide quality percentage composition is 0.5 ~ 5%;
⑵ join any additive in above-mentioned in the alkaline Woolen-making liquid, obtains Wool-making agent, and wherein the volume ratio between additive and the alkaline Woolen-making liquid is 2 ~ 10:100.
Preferred said sodium hydroxide quality percentage composition is 1.5%.
The method of a kind of monocrystalline silicon piece alkali making herbs into wool comprises the steps: the used for solar batteries monocrystalline silicon piece is immersed in and carries out making herbs into wool in the above-mentioned Wool-making agent, and during making herbs into wool, temperature is controlled at 75 ~ 85 ℃, and the making herbs into wool time is 15 ~ 18min.
The present invention is through increase adding auxiliary agent to reach the exposure rate that promotes Si and-OH in solution; Dosing just need not added Virahol with the whole making herbs into wool process of production; The product that does not exist phenomenons such as bubble adhesion, silicon chip is floating, silicon chip is beated to bring is bad, thereby the stabilizing solution system prolongs the solution exhaustion run; Stabilization process is widened the process allowance scope.Making herbs into wool additive of the present invention joins in the Woolen-making liquid, can obtain silicon chip surface matte " pyramid " size evenly, and silicon chip surface does not have finger-marks, no hickie, has reached good making herbs into wool effect.
Meliority of the present invention is:
1. the making herbs into wool additive contains the X 2073 tensio-active agent; Its adding can improve the wettability of Woolen-making liquid and silicon chip surface; And the making herbs into wool additive has shock absorption from corrosive fluid to the transport process of reaction interface to OH-ion in the corrosive fluid; When making corrosion processing silicon single crystal pyramid matte in enormous quantities, NaOH content has the processing range of broad in the solution, helps improving product processes quality of stability.
2. the tensio-active agent in the making herbs into wool additive can be eliminated surperficial finger-marks, eliminates the surface inorganic thing, can reduce the surface tension of solution, makes the making herbs into wool reaction more even, thereby can be so that silicon chip generates fine and closely woven, uniform pyramid.
3. whole process need not added Virahol, can reduce the consumption of conventional organic solvent Virahol, significantly reduces operating environment pollution and wastewater treatment expense that solvent evaporates causes, reduces COD and production cost.
4. adopt thanomin to make corrosion inhibitor, controls reaction speed reduces silicon chip erosion degree effectively; Control pyramid size, external normally used 4-TMAH comes controls reaction speed, and 4-ammonium hydroxide toxicity is stronger; Can cause bigger pollution to environment; And thanomin catalysis is easy to remove after finishing, and does not stay any residue, can not impact ecotope basically.
5. after using making herbs into wool additive of the present invention, the silion cell performance improves, and is embodied in: gained matte pyramid size does not have the space between the even and adjacent pyramid of pyramid size between 1 ~ 3 μ m, promptly fraction of coverage is high, can obtain lower reflectivity.
6. making herbs into wool additive provided by the invention and method of use are applicable to the silicon chip of solar cell making herbs into wool of different size, satisfy the purpose of suitability for industrialized production.
7. making herbs into wool additive provided by the invention and method of use can shorten the making herbs into wool reaction times, and the whole making herbs into wool time is 15 ~ 18min, and (the common process time is 25 ~ 30min), and production efficiency improves than common process time weak point.
8. use making herbs into wool additive provided by the invention, only need time standby stirring rod in the beginning dosing to mix up feed liquid is mixed to get final product, in the making herbs into wool process, do not need bubbling or recycle pump in the texturing slot, practiced thrift energy consumption.
Embodiment
Through specific embodiment the present invention is described further below, but the present invention is not limited by following examples.
Embodiment 1: (1) additive preparation, 15mol thanomin, 10mol tripoly phosphate sodium STPP, 5mol X 2073,2mol sodium hydroxide are joined in the 90mol deionized water, and mix and be made into the making herbs into wool additive.(2) prepare alkaline Woolen-making liquid, sodium hydroxide is dissolved in the deionized water, obtain alkaline Woolen-making liquid, wherein sodium hydroxide quality percentage composition is 1.5%.The additive 8L for preparing is added in the 100L alkalescence Woolen-making liquid, obtains Wool-making agent.The used for solar batteries monocrystalline silicon piece is immersed in carries out making herbs into wool in the Wool-making agent; During making herbs into wool, temperature is controlled at 80 ℃, and the making herbs into wool time is 17min; It is that 1-3 μ m and size are even that the silicon chip of gained detects pyramid matte size through ESEM; Do not have the space between the adjacent pyramid, reflectivity is 10.0%, and silicon chip single face corrosion thinning amount is 5.5 μ m.
Embodiment 2: (1) additive preparation, 15mol thanomin, 10mol tripoly phosphate sodium STPP, 5mol X 2073,2mol sodium hydroxide are joined in the 90mol deionized water, and mix and be made into the making herbs into wool additive.(2) prepare alkaline Woolen-making liquid, sodium hydroxide is dissolved in the deionized water, obtain alkaline Woolen-making liquid, wherein sodium hydroxide quality percentage composition is 1.5%.The additive 8L for preparing is added in the 100L alkalescence Woolen-making liquid, obtains Wool-making agent.The used for solar batteries monocrystalline silicon piece is immersed in carries out making herbs into wool in the Wool-making agent; During making herbs into wool, temperature is controlled at 75 ℃, and the making herbs into wool time is 15min; It is that 1-2 μ m and size are even that the silicon chip of gained detects pyramid matte size through ESEM; Do not have the space between the adjacent pyramid, reflectivity is 10.9%, and silicon chip single face corrosion thinning amount is 4.5 μ m.
Embodiment 3: (1) additive preparation, 20mol thanomin, 12mol Potassium tripolyphosphate, 8mol X 2073,3mol sodium hydroxide are joined in the 100mol deionized water, and mix and be made into the making herbs into wool additive.(2) prepare alkaline Woolen-making liquid, sodium hydroxide is dissolved in the deionized water, obtain alkaline Woolen-making liquid, wherein sodium hydroxide quality percentage composition is 1.5%.The additive 10L for preparing is added in the 100L alkalescence Woolen-making liquid, obtains Wool-making agent.The used for solar batteries monocrystalline silicon piece is immersed in carries out making herbs into wool in the Wool-making agent; During making herbs into wool, temperature is controlled at 80 ℃, and the making herbs into wool time is 17min; It is that 1-2 μ m and size are even that the silicon chip of gained detects pyramid matte size through ESEM; Do not have the space between the adjacent pyramid, reflectivity is 11.3%, and silicon chip single face corrosion thinning amount is 4.6 μ m.
Embodiment 4: (1) additive preparation, 20mol thanomin, 12mol Potassium tripolyphosphate, 8mol X 2073,3mol sodium hydroxide are joined in the 100mol deionized water, and mix and be made into the making herbs into wool additive.(2) prepare alkaline Woolen-making liquid, sodium hydroxide is dissolved in the deionized water, obtain alkaline Woolen-making liquid, wherein sodium hydroxide quality percentage composition is 1.5%.The additive 10L for preparing is added in the 100L alkalescence Woolen-making liquid, obtains Wool-making agent.The used for solar batteries monocrystalline silicon piece is immersed in carries out making herbs into wool in the Wool-making agent; During making herbs into wool, temperature is controlled at 85 ℃, and the making herbs into wool time is 18min; It is that 1-2 μ m and size are even that the silicon chip of gained detects pyramid matte size through ESEM; Do not have the space between the adjacent pyramid, reflectivity is 10.9%, and silicon chip single face corrosion thinning amount is 5 μ m.
Embodiment 5: (1) additive preparation, 12mol thanomin, 8mol ammonium polyphosphate (n=10), 3mol X 2073,1mol sodium hydroxide are joined in the 80mol deionized water, and mix and be made into the making herbs into wool additive.(2) prepare alkaline Woolen-making liquid, sodium hydroxide is dissolved in the deionized water, obtain alkaline Woolen-making liquid, wherein sodium hydroxide quality percentage composition is 1.5%.The additive 2L for preparing is added in the 100L alkalescence Woolen-making liquid, obtains Wool-making agent.The used for solar batteries monocrystalline silicon piece is immersed in carries out making herbs into wool in the Wool-making agent; During making herbs into wool, temperature is controlled at 80 ℃, and the making herbs into wool time is 17min; It is that 2-7 μ m and size are even that the silicon chip of gained detects pyramid matte size through ESEM; Do not have the space between the adjacent pyramid, reflectivity is 11.5%, and silicon chip single face corrosion thinning amount is 6 μ m.
Embodiment 6: (1) additive preparation, 12mol thanomin, 8mol ammonium polyphosphate (n=20), 3mol X 2073,1mol sodium hydroxide are joined in the 80mol deionized water, and mix and be made into the making herbs into wool additive.(2) prepare alkaline Woolen-making liquid, sodium hydroxide is dissolved in the deionized water, obtain alkaline Woolen-making liquid, wherein sodium hydroxide quality percentage composition is 1.5%.The additive 2L for preparing is added in the 100L alkalescence Woolen-making liquid, obtains Wool-making agent.The used for solar batteries monocrystalline silicon piece is immersed in carries out making herbs into wool in the Wool-making agent; During making herbs into wool, temperature is controlled at 75 ℃, and the making herbs into wool time is 15min; It is that 2-3 μ m and size are even that the silicon chip of gained detects pyramid matte size through ESEM; Do not have the space between the adjacent pyramid, reflectivity is 11.3%, and silicon chip single face corrosion thinning amount is 5.8 μ m.
Embodiment 7: (1) additive preparation, 15mol thanomin, 10mol tripoly phosphate sodium STPP, 5mol X 2073,2mol sodium hydroxide are joined in the 90mol deionized water, and mix and be made into the making herbs into wool additive.(2) prepare alkaline Woolen-making liquid, sodium hydroxide is dissolved in the deionized water, obtain alkaline Woolen-making liquid, wherein sodium hydroxide quality percentage composition is 2.0%.The additive 8L for preparing is added in the 100L alkalescence Woolen-making liquid, obtains Wool-making agent.The used for solar batteries monocrystalline silicon piece is immersed in carries out making herbs into wool in the Wool-making agent; During making herbs into wool, temperature is controlled at 80 ℃, and the making herbs into wool time is 17min; It is that 3-5 μ m and size are even that the silicon chip of gained detects pyramid matte size through ESEM; Do not have the space between the adjacent pyramid, reflectivity is 10.8%, and silicon chip single face corrosion thinning amount is 6.5 μ m.
Embodiment 8: (1) additive preparation, 20mol thanomin, 12mol Potassium tripolyphosphate, 8mol X 2073,3mol sodium hydroxide are joined in the 100mol deionized water, and mix and be made into the making herbs into wool additive.(2) prepare alkaline Woolen-making liquid, sodium hydroxide is dissolved in the deionized water, obtain alkaline Woolen-making liquid, wherein sodium hydroxide quality percentage composition is 1.0%.The additive 10L for preparing is added in the 100L alkalescence Woolen-making liquid, obtains Wool-making agent.The used for solar batteries monocrystalline silicon piece is immersed in carries out making herbs into wool in the Wool-making agent, during making herbs into wool, temperature is controlled at 80 ℃; The making herbs into wool time is 17min; It is that 1-2 μ m and size are even that the silicon chip of gained detects pyramid matte size through ESEM, does not have the space between the adjacent pyramid, and some pyramid has just gone out suede; Reflectivity is 11.0%, and silicon chip single face corrosion thinning amount is 4.1 μ m.
Embodiment 9: (1) additive preparation, 12mol thanomin, 8mol ammonium polyphosphate (n=15), 3mol X 2073,1mol sodium hydroxide are joined in the 80mol deionized water, and mix and be made into the making herbs into wool additive.(2) prepare alkaline Woolen-making liquid, sodium hydroxide is dissolved in the deionized water, obtain alkaline Woolen-making liquid, wherein sodium hydroxide quality percentage composition is 1.8%.The additive 2L for preparing is added in the 100L alkalescence Woolen-making liquid, obtains Wool-making agent.The used for solar batteries monocrystalline silicon piece is immersed in carries out making herbs into wool in the Wool-making agent; During making herbs into wool, temperature is controlled at 80 ℃, and the making herbs into wool time is 17min; It is that 2-6 μ m and size are even that the silicon chip of gained detects pyramid matte size through ESEM; Do not have the space between the adjacent pyramid, reflectivity is 11.5%, and silicon chip single face corrosion thinning amount is 6.3 μ m.
In a word, the present invention is used for the mol ratio between each component of additive of monocrystalline silicon piece alkali making herbs into wool and coordinates mutually with volume, temperature of reaction, the reaction times of Woolen-making liquid.The additive that adopts the present invention to be used for the making herbs into wool of monocrystalline silicon piece alkali can shorten the making herbs into wool reaction times, improves production capacity, and made matte pyramid size is even, and reflectivity is low, is applicable to the silicon chip of solar cell alkali making herbs into wool of different size, satisfies the purpose of suitability for industrialized production.
The foregoing description only is used to the inventive concept of the present invention of explaining, but not to the qualification of rights protection of the present invention, allly utilizes this design that the present invention is carried out the change of unsubstantiality, all should fall into protection scope of the present invention.
Claims (8)
1. an additive that is used for the making herbs into wool of monocrystalline silicon piece alkali is characterized in that by following component formulated: thanomin, poly-phosphate, X 2073, sodium hydroxide, water.
2. a kind of additive that is used for the making herbs into wool of monocrystalline silicon piece alkali as claimed in claim 1 is characterized in that: the mol ratio between said thanomin, poly-phosphate, X 2073, sodium hydroxide, the water is 12 ~ 25:5 ~ 15:1 ~ 10:1 ~ 5:20 ~ 100.
3. a kind of additive that is used for the making herbs into wool of monocrystalline silicon piece alkali as claimed in claim 2 is characterized in that: the mol ratio between said thanomin, poly-phosphate, X 2073, sodium hydroxide, the water is 15 ~ 20:8 ~ 12:3 ~ 8:1 ~ 3:80 ~ 100.
4. like claim 1 or 2 or 3 described a kind of additives that are used for the making herbs into wool of monocrystalline silicon piece alkali, it is characterized in that: said water is deionized water.
5. like claim 1 or 2 or 3 described a kind of additives that are used for the making herbs into wool of monocrystalline silicon piece alkali, it is characterized in that: said poly-phosphate can be any one in Rapisol, sodium polyphosphate, the ammonium polyphosphate.
6. Wool-making agent that is used for the making herbs into wool of monocrystalline silicon piece alkali is characterized in that by following steps formulated:
⑴ be dissolved in sodium hydroxide in the deionized water, obtains alkaline Woolen-making liquid, and wherein sodium hydroxide quality percentage composition is 0.5 ~ 5%;
⑵ join any additive among the claim 1-5 in the alkaline Woolen-making liquid, obtains Wool-making agent, and wherein the volume ratio between additive and the alkaline Woolen-making liquid is 2 ~ 10:100.
7. a kind of Wool-making agent that is used for the making herbs into wool of monocrystalline silicon piece alkali as claimed in claim 6 is characterized in that: said sodium hydroxide quality percentage composition is 1.5%.
8. the method for monocrystalline silicon piece alkali making herbs into wool is characterized in that comprising the steps: the used for solar batteries monocrystalline silicon piece is immersed in the Wool-making agent of claim 6 and carries out making herbs into wool, and during making herbs into wool, temperature is controlled at 75 ~ 85 ℃, and the making herbs into wool time is 15 ~ 18min.
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